气相色谱-质谱法分析土壤中十溴联苯醚

通过优化分析仪器的条件设置,建立了使用气相色谱-质谱技术分析十溴联苯醚(BDE 209)的仪器分析方法。通过实施严格的质量控制和质量保证(QA/QC)措施,建立了使用加速溶剂萃取(ASE)技术测试土壤中十溴联苯醚的分析检测方法。该方法的仪器检出限为9.75pg,方法检出限3.25ng/g,方法的精密度为5.56%,平均回收率为86.8%。比较了加速溶剂萃取、微波萃取、超声萃取、索氏抽提等方法的萃取回收效率,实验结果表明,四种方法的萃取回收率在97.7%~108%,都可以作为分析检测土壤中BDE 209的萃取方法。

Determination of Deca Brominated Diphenyl Ether in Soil Sample by Gas Chromatography-Mass Spectrometry

A gas chromatography-mass spectrometric method for determination of deca brominated diphenyl ether(BDE 209) was developed by optimizing the instrumental operating conditions.In addition,a sample preparation method for determination of BDE 209 in soils by accelerated solvent extraction(ASE) was investigated based on the strict QA/QC protocols.The detection limits of the instrumental and the method were 9.75 pg and 3.25 ng/g respectively.The mean recovery was 86.8% with precision of 5.56%RSD.The surrogate standards were used in comparison of extraction efficiency for ASE,microwave extraction,ultrasonic extraction and Soxhlet extraction techniques and the results showed that the similar recovery of 97.7%～108% was obtained,which means that all the extraction methods mentioned above are suitable for determination of BDE 209 in soil samples.